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2,3-Dihydroxybutanedioic Acid → N-t-Butyl-3-formylandrosta-3,5-diene-17beta-carboxamide

HRID 962698
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HRID 962698 반응식
[H-].C([Al+]CC(C)C)C(C)C.[C:11]([NH:15][C:16]([C@H:18]1[CH2:23][CH2:22][C@H:21]2[C@H:24]3[C@H:34]([CH2:35][CH2:36][C@:19]12[CH3:20])[C@:32]1([CH3:33])[C:27]([CH:28]=[C:29]([C:37]#N)[CH2:30][CH2:31]1)=[CH:26][CH2:25]3)=[O:17])([CH3:14])([CH3:13])[CH3:12].C(O)(=O)C(C(C(O)=O)O)[OH:41]>C1(C)C=CC=CC=1>[C:11]([NH:15][C:16]([C@H:18]1[CH2:23][CH2:22][C@H:21]2[C@H:24]3[C@H:34]([CH2:35][CH2:36][C@:19]12[CH3:20])[C@:32]1([CH3:33])[C:27]([CH:28]=[C:29]([CH:37]=[O:41])[CH2:30][CH2:31]1)=[CH:26][CH2:25]3)=[O:17])([CH3:12])([CH3:13])[CH3:14]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8752,3-Dihydroxybutanedioic AcidHCID 21225700DiisobutylaluminumhydrideHCID 676469513-Cyano-N-(1,1-dimethylethyl)androsta-3,5-diene-17-beta-carboxamide

생성물 1

HCID 86749645N-t-Butyl-3-formylandrosta-3,5-diene-17beta-carboxamide

시약·촉매·용매 1

HCID 1140Toluene용매2회

반응 조건

온도
0 °C

실험 절차

2 ml of a 1M solution of diisobutyl aluminum hydride in toluene were added at 0° C. to 10 ml of a dry solution of toluene containing 380 mg of N-t-butyl-3-cyanoandrosta-3,5-diene-17β-carboxamide (prepared as described in Preparation 2). The reaction mixture was then stirred at 0° C. for 30 minutes, after which 30 ml of an aqueous solution of 1.5 g of tartaric acid were added to the mixture. The reaction mixture was then stirred at room temperature for 2 hours, and then extracted with methylene chloride three times. The combined organic extracts were washed with water and with a saturated aqueous solution of sodium chloride, in that order. They were then dried over anhydrous magnesium sulfate, and concentrated by evaporation under reduced pressure. The resulting residue was subjected to column chromatography using 50 g of silica gel and using a gradient elution method, with mixtures of acetone and methylene chloride in ratios ranging from 1:99 to 4:96 by volume as the eluent, to give 325 mg of the title compound.

후처리

  1. stirringThe reaction mixture was then stirred at room temperature for 2 hours
  2. extractionextracted with methylene chloride three times
  3. washThe combined organic extracts were washed with water and with a saturated aqueous solution of sodium chloride, in that order
  4. dry with materialThey were then dried over anhydrous magnesium sulfate
  5. concentrationconcentrated by evaporation under reduced pressure
  6. washa gradient elution method

출처 및 근거

ORD 기록
ord-80f184ecd11049a8a528b719e688d85d
출처 데이터셋
uspto-grants-1998_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05760025

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